Metal doped mesoporous silicon-based molecular sieve nanosphere and preparation method thereof

A technology of metal doping and molecular sieve, applied in the direction of crystalline aluminosilicate zeolite, etc., to achieve the effect of easy industrial production, safe operation and lower production cost

Active Publication Date: 2014-12-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Within the scope of the applicant's search, there is no report on the direct synthesis of MSN-M molecular sieve nanospheres using the two-step process of the sol-gel method

Method used

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  • Metal doped mesoporous silicon-based molecular sieve nanosphere and preparation method thereof
  • Metal doped mesoporous silicon-based molecular sieve nanosphere and preparation method thereof
  • Metal doped mesoporous silicon-based molecular sieve nanosphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 Synthesis of zirconium-doped mesoporous silicon-based molecular sieve nanospheres

[0025]Ethyl orthosilicate is used as the silicon source, and zirconium n-propoxide is used as the zirconium source. Dilute 12g of concentrated ammonia water (25wt%) to 300g (pH=11.4) with deionized water, add 0.58g of CTAB, stir and dissolve in a 50°C water bath. Prepare ethanol solution A of ethyl orthosilicate with different concentrations and ethanol mixed solution B of ethyl orthosilicate and zirconium n-propoxide: the concentration of (Si) in A is 0.2mol L -1 , the concentration of (Si) in B is 1.0mol·L -1 (At the same time, B prepared three groups respectively, so that Zr / Si=0.025, 0.05, 0.1). Quickly add 5mL of solution A to the above mixture under stirring, seal the reactor, stir for 5 hours, open the reactor, add 5mL of solution B dropwise, continue stirring for 1 hour, stop stirring, and stand in a water bath at 50°C for 20 hours. The reaction mixture was separated...

Embodiment 2

[0026] Example 2 Effect of different molar ratios of CTAB on the synthesis of zirconium-doped mesoporous silicon-based molecular sieve nanospheres

[0027] Ethyl orthosilicate is used as the silicon source, and zirconium n-propoxide is used as the zirconium source. Dilute 12g of concentrated ammonia water (25wt%) to 300g (pH=11.4) with deionized water, add 0.50g, 0.58g, 0.70g of CTAB respectively, stir and dissolve in a 50°C water bath. Prepare ethanol solution A of ethyl orthosilicate with different concentrations and ethanol mixed solution B of ethyl orthosilicate and zirconium n-propoxide: the concentration of (Si) in A is 0.2mol L -1 , the concentration of (Si) in B is 1.0mol·L -1 ; Zr / Si=0.05 in B. Quickly add 5mL of solution A to the above mixture under stirring, seal the reactor, stir for 5 hours, open the reactor, add 5mL of solution B dropwise, continue stirring for 1 hour, stop stirring, and stand in a water bath at 50°C for 20 hours. The reaction mixture was cent...

Embodiment 3

[0028] Example 3 Different templates are used to synthesize titanium-doped mesoporous silicon-based molecular sieve nanospheres

[0029] Ethyl orthosilicate is used as the silicon source, and titanium tetrachloride is used as the titanium source. Dilute 12g of concentrated ammonia water (25wt%) to 300g (pH=11.4) with deionized water, add 0.42g of DTAC, 0.58g of CTAB, and 0.55g of STAC, and stir to dissolve in a 50°C water bath. Prepare ethanol solutions A of different concentrations of ethyl orthosilicate and ethanol mixed solution B of ethyl orthosilicate and titanium tetrachloride: the concentration of (Si) in A is 0.2mol L -1 , the concentration of (Si) in B is 1.0mol·L -1 ; Ti / Si=0.05 in B. Quickly add 5mL of solution A to the above mixture under stirring, seal the reactor, stir for 5 hours, open the reactor, add 5mL of solution B dropwise, continue stirring for 1 hour, stop stirring, and stand in a water bath at 50°C for 20 hours. The reaction mixture was separated by ...

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Abstract

The invention discloses a metal doped mesoporous silicon-based molecular sieve nanosphere and a preparation method thereof. The doped metal ion is one or more than two of IA, IIA, IIIA, VA, VIA, excess metal and rare earth metal in a periodic table, the mole ratio of the doped metal ion to silicon ion is 0.01 to 0.2; a nanosphere material has an uniform hexagonal tunnel structure, the average granularity is 60-200nm, specific surface area is 600-1600m<2>.g<-1>, and mesoporous aperture is 2.0-3.0nm. According to the invention, common silicon source, metal source and a surfactant are taken as raw materials, an alkalescence medium is used for adjusting pH value of a reaction mixture, a sol-gel method is used for direct synthesis of the metal doped mesoporous silicon-based molecular sieve nanosphere (MSN-M) material. The method has the advantages of simple technology and safe operation, continuous adjustment of pH value is not required, thermal crystallisation process under high pressure water and high temperature is not required, raw materials are easy to obtain, and the industrial production is easy.

Description

technical field [0001] The invention relates to the field of inorganic porous materials, in particular to mesoporous silicon-based nanomaterials, more specifically a metal-doped mesoporous silicon-based molecular sieve nanosphere and a preparation method thereof. Background technique [0002] As a new type of inorganic solid porous material, silicon-based mesoporous molecular sieve has the characteristics of high specific surface, regular channels, large pore volume, adjustable pore size of 2-50nm, and physical adsorption or chemical modification on the surface of the channels. Adsorption separation, biomedicine, functional materials and other fields have broad application prospects. In 1992, Mobil Corporation first publicly reported the M41S mesoporous silica material [J.Am.Chem.Soc.1992,114,10834] Subsequently, HMS, MSU, KIT-1, SBA and their heteroatomized series of mesoporous molecular sieves continued to See reports. In recent years, the development of nano molecular s...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 徐杰陈佳志路芳张俊杰于维强高进苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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